CN109772305A - A kind of metallic substrates carried noble metal integral catalyzer and its one-step preppn process and application - Google Patents
A kind of metallic substrates carried noble metal integral catalyzer and its one-step preppn process and application Download PDFInfo
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- CN109772305A CN109772305A CN201910020342.2A CN201910020342A CN109772305A CN 109772305 A CN109772305 A CN 109772305A CN 201910020342 A CN201910020342 A CN 201910020342A CN 109772305 A CN109772305 A CN 109772305A
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Abstract
The invention belongs to air purification field, a kind of metallic substrates carried noble metal integral catalyzer and its one-step preppn process and application are disclosed.The following steps are included: metal aluminum substrate is put into noble metal precursor liquid solution, 0.5-3h is persistently stirred to react in 40-60 DEG C of water-bath, then by sample taking-up distilled water flushing it is clean after, in 120 DEG C of dry 3h；Noble metal precursor liquid solution is the solution containing palladium chloride and/or chloroplatinic acid, and solvent is water.The present invention is not necessarily to before carried noble metal active component carry out the modified pretreatment in surface to metallic matrix using special techniques such as anodic oxidations, the modified in-situ deposition with noble metal active component in surface of metallic matrix need to be only completed at the same time by simple one-step method process, i.e. while making metal base surface form convex-concave fluctuating and there is the thin layer of metal oxide of certain hole configurations, completes noble metal active component particle in-situ deposition in the thin layer of formation and load.
Description
Technical field
The invention belongs to air purification field, in particular to a kind of metallic substrates carried noble metal integral catalyzer and
Its one-step method preparation method and application.
Background technique
Volatile organic compounds (VOCs) is a kind of important atmosphere pollution, can not only cause prestige to human health
The side of body, and also have serious harm to ecological environment.As one of processing VOCs most efficient method, the side of catalytic oxidation combustion
Formula has many advantages, such as high burning efficiency, without secondary pollution, and this method it is most crucial be catalyst.Support type integral catalyzer
It is one of the important catalyst system of catalytic oxidation combustion process study, the active component used is generally divided into precious metal catalyst
Agent and non-precious metal catalyst.Wherein, noble metal catalyst has lower initiation temperature and low-temperature catalyzed purification efficiency height etc.
Advantage, but it is expensive, therefore prepare noble metal monolithic catalyst and key problems-solving is needed to be, how to guarantee preferably
On the basis of catalytic activity, simplifies preparation process as far as possible and reduce noble metal dosage, to reduce catalyst cost.
Commonly regular carrier mainly has metallic matrix (such as wire mesh and metal beehive to support type integral catalyzer
Deng) and two kinds of ceramic matrix (such as ceramic honeycomb).Compared to ceramic matrix, metallic matrix has higher heat conductivity, stronger
Machinability and higher shock resistance the advantages that, therefore low temperature purification is more efficient, and the scope of application is more extensive.But Metal Substrate body surface
Face is usually smooth non-porous, is unfavorable for noble metal active component and is uniformly distributed on its surface and securely loads.Therefore current preparation gold
When belonging to matrix carried noble metal integral catalyzer, it usually needs before infusion process carried noble metal step, increase Metal Substrate
The bright pre-treatment step of body surface, i.e., using anodizing technology, electrophoretic deposition technique or high-temperature heat treatment technology etc. in metallic matrix
Surface is initially formed the high and porous metal-oxide film of one layer of dense uniform, adhesive force, is just more advantageous to subsequent step in this way
Middle noble metal is uniformly distributed in the metal-oxide film of formation and securely loads.This results in current metallic matrix support type
The preparation process of noble metal monolithic catalyst is excessively cumbersome, energy consumption is high, preparation cost is high, is unfavorable for scale application.
Summary of the invention
In order to overcome shortcoming and deficiency existing in the prior art, the primary purpose of the present invention is that providing a kind of Metal Substrate
It is thin to form metal oxide in metal base surface modification for the one-step preppn process of bed load type noble metal monolithic catalyst
While layer, noble metal active component particle also completes in-situ deposition load in the thin layer of formation.
Another object of the present invention is to provide a kind of loads of metallic substrates that above-mentioned one-step preppn process is prepared
Type noble metal monolithic catalyst.
A further object of the present invention is to provide a kind of answering for above-mentioned metallic substrates carried noble metal integral catalyzer
With.
The object of the invention is achieved through the following technical solutions:
A kind of one-step preppn process of metallic substrates carried noble metal integral catalyzer, comprising the following steps: will
Metallic matrix is put into noble metal precursor liquid solution, and 0.5-3h is persistently stirred to react in 40-60 DEG C of water-bath, then takes sample
Out with distilled water flushing it is clean after, in 120 DEG C of dry 3h；
The metallic matrix is metallic aluminium；
The noble metal precursor liquid solution is the solution containing palladium chloride and/or chloroplatinic acid, and solvent is water.
The metallic matrix is metal aluminum honeycomb, metal aluminium flake or metal aluminum foil.
The concentration of the palladium chloride in the solution is 0.2-7.6mg/L, and the concentration of the chloroplatinic acid in the solution is 0.2-
2.2mg/L。
Also contain ammonium hydroxide, ammonium chloride, sodium hypophosphite and/or hydrazine hydrate in the noble metal precursor liquid solution.
The additional amount of the ammonium hydroxide in the solution is 50-100mL/L, and the concentration of the ammonium chloride in the solution is 5.0-
13.5g/L, the concentration of the sodium hypophosphite in the solution are 2.0-5.0g/L, and it is 2mol/L that the hydrazine hydrate, which is by concentration,
Hydrazine hydrate is added in solution with the additional amount of 40-70mL/L.
A kind of metallic substrates carried noble metal monoblock type catalysis being prepared according to above-mentioned one-step preppn process
Agent.
Application of the above-mentioned metallic substrates carried noble metal integral catalyzer in purification of volatile organic pollutant.
Compared with prior art, the present invention has the following advantages and beneficial effects:
The method of the present invention, relative to general metallic matrix carried noble metal integral catalyzer preparation method and
Speech, without carrying out the modified pre- place in surface to metallic matrix using special techniques such as anodic oxidations before carried noble metal active component
Reason, the surface that metallic matrix need to be only completed at the same time by simple one-step method process are modified heavy with the original position of noble metal active component
Product, i.e., it is complete while making metal base surface form convex-concave fluctuating and there is the thin layer of metal oxide of certain hole configurations
At noble metal active component particle, in-situ deposition is loaded in the thin layer of formation；It is burnt simultaneously using monoblock type produced by the present invention
Catalyst, can (0.02-0.20wt.%) very low in bullion content under the conditions of, excellent VOCs low temperature combustion can be shown
It burns purifying property: in 168-225 DEG C of ignition, reaching at 231-288 DEG C and be fully cleaned up；Preparation method provided by the invention implements step
Rapid simple, easy to operate, obtained catalyst prod is cheap and catalytic purification superior activity, and there is good market to answer
With value and promotion prospect.
Detailed description of the invention
Fig. 1 is the EDS elemental analysis result schematic diagram of blank metal aluminium flake used in embodiment 1.
Fig. 2 is the SEM surface microscopic topographic figure of blank metal aluminium flake used in embodiment 1.
Fig. 3 is the EDS elemental analysis result schematic diagram of obtained catalyst sample in embodiment 1.
Fig. 4 is the SEM surface microscopic topographic figure of obtained catalyst sample in embodiment 1.
Fig. 5 is the EDS elemental analysis result schematic diagram of obtained catalyst sample in embodiment 8.
Fig. 6 is the SEM surface microscopic topographic figure of obtained catalyst sample in embodiment 8, wherein (a) is enlargement ratio
50k times；It (b) is 300k times of enlargement ratio.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail, and embodiments of the present invention are not limited thereto.
Embodiment 1:
By length and width and with a thickness of 50 × 12 × 0.05mm and quality is the metal aluminium flake of 0.16g, is put into noble metal precursor body
In solution, be persistently stirred to react 2h in 50 DEG C of water-baths, then by sample taking-up distilled water flushing it is clean after, it is dry at 120 DEG C
Dry 3h, obtains integral catalyzer.Wherein noble metal precursor liquid solution contains the palladium chloride of 3.2mg/L, the ammonium hydroxide of 100mL/L,
The ammonium chloride of 13.5g/L and the sodium hypophosphite of 5.0g/L.
The mass content of precious metals pd is 0.10% in the integral catalyzer sample that the present embodiment obtains, for toluene
Catalytic oxidation combustion purification Activity evaluation be shown in Table 1.
Embodiment 2:
By length and width and with a thickness of 50 × 12 × 0.05mm and quality is the metal aluminium flake of 0.16g, is put into noble metal precursor body
In solution, be persistently stirred to react 0.5h in 50 DEG C of water-baths, then by sample taking-up distilled water flushing it is clean after, at 120 DEG C
Dry 3h, obtains integral catalyzer.Wherein noble metal precursor liquid solution contains the palladium chloride of 1.6mg/L, the ammonium hydroxide of 80mL/L,
The ammonium chloride of 10g/L and the sodium hypophosphite of 3.0g/L.
The mass content of precious metals pd is 0.05% in the integral catalyzer sample that the present embodiment obtains, for toluene
Catalytic oxidation combustion purification Activity evaluation be shown in Table 1.
Embodiment 3:
By length and width and with a thickness of 12 × 29 × 0.2mm and quality is the metal aluminium flake of 0.19g, is put into noble metal precursor body
In solution, be persistently stirred to react 3h in 60 DEG C of water-baths, then by sample taking-up distilled water flushing it is clean after, it is dry at 120 DEG C
Dry 3h, obtains integral catalyzer.Wherein noble metal precursor liquid solution contains the palladium chloride of 7.6mg/L, the ammonium hydroxide of 100mL/L,
The ammonium chloride of 13.5g/L and the sodium hypophosphite of 5.0g/L.
The mass content of precious metals pd is 0.20% in the integral catalyzer sample that the present embodiment obtains, for toluene
Catalytic oxidation combustion purification Activity evaluation be shown in Table 1.
Embodiment 4:
By length and width and with a thickness of 12 × 150 × 0.02mm and quality is the metal aluminum foil of 0.11g, is put into noble metal precursor
In liquid solution, be persistently stirred to react 3h in 50 DEG C of water-baths, then by sample taking-up distilled water flushing it is clean after, at 120 DEG C
Dry 3h, obtains integral catalyzer.Wherein noble metal precursor liquid solution contains the palladium chloride of 4.4mg/L, the ammonia of 100mL/L
Water, the ammonium chloride of 13.5g/L and the sodium hypophosphite of 5.0g/L.
The mass content of precious metals pd is 0.20% in the integral catalyzer sample that the present embodiment obtains, for toluene
Catalytic oxidation combustion purification Activity evaluation be shown in Table 1.
Embodiment 5:
By the metal aluminum honeycomb that length and width is 5 × 4.5 × 20mm with height and quality is 0.11g, it is put into noble metal precursor body
In solution, be persistently stirred to react 2h in 50 DEG C of water-baths, then by sample taking-up distilled water flushing it is clean after, it is dry at 120 DEG C
Dry 3h, obtains integral catalyzer.Wherein noble metal precursor liquid solution contains the palladium chloride of 2.2mg/L, the ammonium hydroxide of 80mL/L,
The ammonium chloride of 11g/L and the sodium hypophosphite of 4.0g/L.
The mass content of precious metals pd is 0.10% in the integral catalyzer sample that the present embodiment obtains, for toluene
Catalytic oxidation combustion purification Activity evaluation be shown in Table 1.
Embodiment 6:
By the metal aluminum honeycomb that length and width is 5 × 4.5 × 20mm with height and quality is 0.11g, it is put into noble metal precursor body
In solution, be persistently stirred to react 0.5h in 40 DEG C of water-baths, then by sample taking-up distilled water flushing it is clean after, at 120 DEG C
Dry 3h, obtains integral catalyzer.Wherein noble metal precursor liquid solution contains the palladium chloride of 0.4mg/L, the ammonium hydroxide of 50mL/L,
The ammonium chloride of 5.0g/L and the sodium hypophosphite of 2.0g/L.
The mass content of precious metals pd is 0.02% in the integral catalyzer sample that the present embodiment obtains, for toluene
Catalytic oxidation combustion purification Activity evaluation be shown in Table 1.
Embodiment 7:
By length and width and with a thickness of 50 × 12 × 0.05mm and quality is the metal aluminium flake of 0.16g, is put into noble metal precursor body
In solution, the sustained response 3h in 50 DEG C of water-baths, then by sample taking-up distilled water flushing it is clean after, in 120 DEG C of dry 3h,
Obtain integral catalyzer.Wherein noble metal precursor liquid solution contains the palladium chloride of 3.2mg/L, the ammonium hydroxide and 12g/L of 100mL/L
Ammonium chloride.
The mass content of precious metals pd is 0.10% in the integral catalyzer sample that the present embodiment obtains, for toluene
Catalytic oxidation combustion purification Activity evaluation be shown in Table 1.
Embodiment 8:
By the metal aluminum honeycomb that length and width is 5 × 4.5 × 20mm with height and quality is 0.11g, it is put into noble metal precursor body
In solution, be persistently stirred to react 1.5h in 50 DEG C of water-baths, then by sample taking-up distilled water flushing it is clean after, at 120 DEG C
Dry 3h, obtains integral catalyzer.Wherein noble metal precursor liquid solution contains the chloroplatinic acid of 2.2mg/L, the ammonia of 100mL/L
Water, the ammonium chloride of 13.5g/L and the hydrazine hydrate of 60mL/L.
The mass content of precious metals pt is 0.10% in the integral catalyzer sample that the present embodiment obtains, for toluene
Catalytic oxidation combustion purification Activity evaluation be shown in Table 1.
Embodiment 9:
By the metal aluminum honeycomb that length and width is 5 × 4.5 × 20mm with height and quality is 0.11g, it is put into noble metal precursor body
In solution, be persistently stirred to react 1.5h in 40 DEG C of water-baths, then by sample taking-up distilled water flushing it is clean after, at 120 DEG C
Dry 3h, obtains integral catalyzer.Wherein noble metal precursor liquid solution contains the chloroplatinic acid of 0.4mg/L, the ammonium hydroxide of 50mL/L
With the ammonium chloride of 6.0g/L.
The mass content of precious metals pt is 0.02% in the integral catalyzer sample that the present embodiment obtains, for toluene
Catalytic oxidation combustion purification Activity evaluation be shown in Table 1.
Embodiment 10:
By the metal aluminum honeycomb that length and width is 5 × 4.5 × 20mm with height and quality is 0.11g, it is put into noble metal precursor body
In solution, be persistently stirred to react 2h in 50 DEG C of water-baths, then by sample taking-up distilled water flushing it is clean after, it is dry at 120 DEG C
Dry 3h, obtains integral catalyzer.Wherein noble metal precursor liquid solution contains the chloroplatinic acid of 0.2mg/L, the chlorination of 0.2mg/L
Palladium, the ammonium hydroxide of 70mL/L and the ammonium chloride of 9.0g/L.
The mass content of precious metals pt and Pd are all 0.01% (to urge in the integral catalyzer sample that the present embodiment obtains
Noble metal gross mass content is that 0.02%), the catalytic oxidation combustion purification Activity evaluation of toluene is shown in Table in agent
1。
Energy is carried out to blank metal matrix used in embodiment 1 and obtained catalyst sample Pd/Al catalyst respectively
Scattered X-rays compose (EDS) elemental analysis, and acquired results are shown in Fig. 1 and Fig. 3 respectively.By Fig. 1, it can be concluded that, blank metal matrix is only
Containing two kinds of elements of Al and O, and the molar ratio of Al and O is very high, about 26:1, this illustrates blank metal matrix mainly by metallic state
Aluminium element is constituted.Further through scanning electron microscope (SEM) analysis result (Fig. 2) as it can be seen that blank metal matrix surface is smooth, and
Without hole.Tri- kinds of elements of Al, O and Pd, and Al and O it can be concluded that, are contained by the EDS result of Fig. 3 in obtained catalyst sample
Molar ratio be reduced to 1.5:1, this aspect illustrates that precious metals pd has been supported on metallic matrix, on the other hand also illustrates gold
Belong to matrix surface part metals state aluminium element and becomes aluminium oxide (Al2O3).Further through sem analysis result (Fig. 4) as it can be seen that institute
Catalyst sample surface, which is made, becomes convex-concave fluctuating and with more hole configurations, this phenomenon and using anodizing technology
The result for carrying out surface preparation to metal aluminum substrate is similar；The spherical nanoparticles of 10-20nm scale are equal in hole simultaneously
Even distribution, without obvious agglomeration.When thus illustrating that metal aluminum substrate and noble metal precursor liquid solution contact, surface metal state aluminium
The alumina flake of convex-concave fluctuating and hole structure is formed by oxidation reaction, while noble metal precursor object is anti-also by reduction
In situ in the form of noble metal nano particles in the alumina flake of formation deposition should be precipitated.
EDS element is carried out to blank metal matrix used in embodiment 8 and obtained catalyst sample Pt/Al catalyst
Analysis, as a result as shown in Figure 1 and Figure 5.As seen from Figure 5, relative to blank metal matrix, in addition to Al in obtained catalyst sample
There are also Pt elements with outside O element, and the molar ratio of Al and O is also reduced to 1.6:1, and this aspect illustrates that precious metals pt has loaded
On metallic matrix, on the other hand also illustrate that metal base surface part metals state aluminium element becomes aluminium oxide (Al2O3).Into
One step is by sem analysis result (Fig. 6) as it can be seen that obtained catalyst sample surface also becomes convex-concave fluctuating and has more hole
Structure, while the spherical nanoparticles of about 10nm scale even compact in hole is distributed, and without obvious reunion stratification.This
One result is identical as Pd/Al catalyst sample obtained.
To other types blank metal matrix used and obtained catalyst sample in embodiment 1-7 and embodiment 9-10
Carry out EDS and SEM test, available phenetic analysis result similar with embodiment 1 and embodiment 8.Offer of the present invention is provided
Integral catalyzer preparation method be suitable on various specifications and the metallic matrix of type use one-step method carried noble metal
Active component prepares monoblock type combustion catalyst.
The integral catalyzer obtained using each embodiment 1-10 (metallic matrix is the loaded noble metal catalyst of carrier)
As catalyst sample, in 300 DEG C of air atmospheres after pre-activate, using the catalysis burning purification of toluene as probe reaction,
Toluene inlet concentration 1.0g/m3With volume space velocity 10000h-1Under the conditions of carry out catalyst activity evaluation, the results are shown in Table 1.Catalyst
Reaction temperature T when activity reaches 10% and 90% with toluene conversion10And T90As evaluation criterion, the lower table of temperature value
Bright catalyst cleaning activity is more outstanding.Seen from table 1, platinum or very low (0.05-0.10wt.%) condition of palladium content in the catalyst
Under, it can be in 168-225 DEG C of low temperature ignition, and reach at 231-288 DEG C and be fully cleaned up, show superior toluene catalytic combustion
Purifying property.This should be attributed to the fact that when preparing integral catalyzer using the present invention, can be in carried noble metal active component
Surface modification treatment, the porous oxidation that such noble metal nano particles can be formed in matrix surface are carried out to metallic matrix simultaneously
Reach evenly dispersed and secured load in object thin layer, to improve its oxidation activity and stability in catalyst combustion reaction.
Catalyst toluene burning purification activity rating is made in 1 embodiment 1-10 of table
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (7)
1. a kind of one-step preppn process of metallic substrates carried noble metal integral catalyzer, it is characterised in that including following
Step: metallic matrix is put into noble metal precursor liquid solution, 0.5-3h is persistently stirred to react in 40-60 DEG C of water-bath, then
By sample taking-up distilled water flushing it is clean after, in 120 DEG C of dry 3h；
The metallic matrix is metallic aluminium；
The noble metal precursor liquid solution is the solution containing palladium chloride and/or chloroplatinic acid, and solvent is water.
2. a kind of one-step method preparation side of metallic substrates carried noble metal integral catalyzer according to claim 1
Method, it is characterised in that: the metallic matrix is metal aluminum honeycomb, metal aluminium flake or metal aluminum foil.
3. a kind of one-step method preparation side of metallic substrates carried noble metal integral catalyzer according to claim 1
Method, it is characterised in that: the concentration of the palladium chloride in the solution is 0.2-7.6mg/L, the concentration of the chloroplatinic acid in the solution
For 0.2-2.2mg/L.
4. a kind of one-step method preparation side of metallic substrates carried noble metal integral catalyzer according to claim 1
Method, it is characterised in that: also contain ammonium hydroxide, ammonium chloride, sodium hypophosphite and/or hydrazine hydrate in the noble metal precursor liquid solution.
5. a kind of one-step method preparation side of metallic substrates carried noble metal integral catalyzer according to claim 4
Method, it is characterised in that: the additional amount of the ammonium hydroxide in the solution is 50-100mL/L, and the concentration of the ammonium chloride in the solution is
5.0-13.5g/L, the concentration of the sodium hypophosphite in the solution are 2.0-5.0g/L, and the hydrazine hydrate is to be by concentration
The hydrazine hydrate of 2mol/L is added in solution with the additional amount of 40-70mL/L.
6. a kind of metallic substrates support type that one-step preppn process according to claim 1-5 is prepared is expensive
Integral type metal catalyst.
7. metallic substrates carried noble metal integral catalyzer according to claim 6 is net in volatile organic contaminant
Application in change.
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